CN115944572A - Toothpaste based on nutgall extract and preparation method thereof - Google Patents
Toothpaste based on nutgall extract and preparation method thereof Download PDFInfo
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- CN115944572A CN115944572A CN202310070298.2A CN202310070298A CN115944572A CN 115944572 A CN115944572 A CN 115944572A CN 202310070298 A CN202310070298 A CN 202310070298A CN 115944572 A CN115944572 A CN 115944572A
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Abstract
The invention relates to the field of daily necessities, in particular to a toothpaste based on a nutgall extract and a preparation method thereof, wherein the toothpaste comprises the following components: the toothpaste disclosed by the invention can be kept in a stable state for a long time in the storage process, has long-acting and lasting antibacterial performance, and has a more lasting effect.
Description
Technical Field
The invention relates to the field of daily necessities, in particular to toothpaste based on a nutgall extract and a preparation method thereof.
Background
A large amount of microorganisms exist in the oral cavity of a human body, if the residual food in the oral cavity is not cleaned in time, harmful bacteria can be rapidly propagated, oral infection and enamel damage can be caused, the teeth can be discolored and yellow, the appearance is influenced, the residual food and the harmful bacteria in the oral cavity can be effectively cleaned through regular tooth brushing, and the health and the sanitation of the oral cavity are maintained.
The toothpaste containing the Chinese herbal medicine components has the mild property and the medicinal effect of the Chinese herbal medicines. Not only can clean the oral cavity and refresh breath, but also can play the roles of clearing away heat and toxic material, inhibiting bacteria and killing bacteria and eliminating inflammation. Galla Turcica is used as a common Chinese medicinal material, and is derived from dried gallnut generated by larva of Commelina guianensis belonging to the family Commelinaceae parasitizing young branch of Commelina guianensis belonging to the family Fagaceae. Gallnut is cold in nature and bitter in taste, has the efficacies of inducing astringency, astringing, eliminating dampness and stopping bleeding, and currently, the application of the gallnut extract in the preparation of toothpaste is rarely reported.
Disclosure of Invention
The invention aims to: aiming at the technical development trend, the invention provides a toothpaste based on a nutgall extract and a preparation method thereof.
The adopted technical scheme is as follows:
a toothpaste based on nutgall extract comprises the following components:
polyethylene glycol, sodium lauryl sulfate, xanthan gum, zinc citrate, cocamidopropyl betaine, galla Turcica extract, fluorine-containing inorganic salt, abrasive, vinyl pyrrolidone-maleic anhydride copolymer, water, and other adjuvants.
Further, the paint comprises the following components in parts by weight:
5-10 parts of polyethylene glycol, 0.5-1.2 parts of sodium lauryl sulfate, 1-2 parts of xanthan gum, 0.2-0.8 part of zinc citrate, 0.1-0.5 part of cocamidopropyl betaine, 2-5 parts of nutgall extract, 0.05-0.15 part of fluorine-containing inorganic salt, 15-30 parts of abrasive, 1-2 parts of vinyl pyrrolidone-maleic anhydride copolymer, 15-20 parts of water and 0-6 parts of other auxiliary materials.
Furthermore, the content of gallic acid in the nutgall extract is more than or equal to 100mg g -1 。
Further, the preparation method of the nutgall extract comprises the following steps:
adding Galla Turcica medicinal powder into methanol water solution, performing oscillation extraction at 40-50 deg.C for 5-10 hr, filtering extractive solution, repeatedly extracting residue, mixing extractive solutions, adding phenyl bonded silica gel into the extractive solution, mixing with dry method, loading into solid phase extraction column tube, compacting, eluting with peristaltic pump, collecting eluate, and vacuum concentrating under reduced pressure.
Further, the eluent comprises methanol and acetic acid, and the volume ratio of the methanol to the acetic acid is 100-120:1.
further, the fluorine-containing inorganic salt is any one or more of sodium fluoride, potassium monofluorophosphate and stannous fluoride.
Further, the abrasive is one or more of calcium hydrogen phosphate dihydrate, calcite powder, precipitated silica, anhydrous calcium pyrophosphate, aluminum hydroxide and titanium dioxide.
Further, the preparation method of the vinylpyrrolidone-maleic anhydride copolymer is as follows:
adding maleic anhydride, vinyl pyrrolidone, azodiisobutyronitrile and divinylbenzene into a mixed solvent consisting of dipropylene glycol dimethyl ether and ethyl acetate, stirring and mixing uniformly, introducing nitrogen for protection, heating to 65-75 ℃, reacting for 6-10h, naturally cooling to room temperature, adding ethanol, stirring for 10-20h, filtering, performing Soxhlet purification on the obtained product for 24-48h by using acetone, washing off unreacted monomers, finally performing vacuum drying to constant weight, and crushing.
Further, the other auxiliary materials comprise any one or more of buffering agent, humectant, edible pigment, antiseptic, essence, sweetener, spice and western medicine components.
The invention also provides a preparation method of the toothpaste based on the nutgall extract, which comprises the following steps:
the preparation method comprises the steps of uniformly mixing polyethylene glycol, sodium lauryl sulfate, cocamidopropyl betaine, a nutgall extract, a vinyl pyrrolidone-maleic anhydride copolymer, water and other auxiliary materials, adding the mixture into a paste making pot, adding zinc citrate powder, fluorine-containing inorganic salt, an abrasive and xanthan gum, stirring, grinding, transferring the mixture into a storage pot, defoaming in vacuum, aging for 24-48h, and filling the mixture into a pipe.
The invention has the beneficial effects that:
the invention provides a toothpaste based on a gallnut extract, wherein the gallnut extract contains gallic acid, methyl gallate, tannin and the like, the inventor finds that the gallnut extract (gallic acid, methyl gallate, tannin and the like) can effectively inhibit the growth of oral bacteria, the inhibition effect of each single component on the oral bacteria is not obvious, and whether the synergistic effect exists between the gallnut extract and the gallnut extract is not very clear, the inventor needs further research, but the gallnut extract can effectively improve the antibacterial performance of the toothpaste, effectively inhibit dental plaque, relieve gingival bleeding and relieve inflammation, a vinyl pyrrolidone-maleic anhydride copolymer can be combined with metal ions in an abrasive to generate corresponding calcium salt or mixed salt, the movement resistance is increased, so that higher viscosity is presented, the consistency and viscosity of the toothpaste are improved, the toothpaste can be kept in a stable state for a long time in the storage process, the release time of the gallnut extract can be prolonged, the antibacterial performance is achieved, and the toothpaste product is more durable.
Drawings
FIG. 1 is a graph showing the comparison of the stain removing effects in example 1 of the present invention;
before A is stain removal and after B is stain removal, the toothpaste prepared by the embodiment has a good stain removal effect.
Detailed Description
The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially. The technology not mentioned in the present invention is referred to the prior art.
Example 1:
the toothpaste based on the nutgall extract comprises the following components in parts by weight:
8 parts of polyethylene glycol, 1 part of sodium lauryl sulfate, 1.5 parts of xanthan gum, 0.6 part of zinc citrate, 0.1 part of cocamidopropyl betaine, 5 parts of nutgall extract, 0.12 part of sodium fluoride, 20 parts of anhydrous calcium pyrophosphate, 1 part of vinyl pyrrolidone-maleic anhydride copolymer and 18 parts of water.
The preparation method of the nutgall extract comprises the following steps:
adding 10g Galla Turcica powder into 80mL methanol water solution (V) Methanol :V Water (W) = 1), heating to 50 ℃, performing oscillation extraction for 8 hours under the action of ultrasonic waves, filtering an extracting solution, repeatedly extracting residues for 1 time, combining the extracting solutions, adding 50g of phenyl bonded silica gel into the extracting solution, uniformly mixing, performing reduced pressure concentration to remove a solvent, filling the obtained powder into a solid-phase extraction column tube, compacting, driving an eluent by using a peristaltic pump to perform elution, wherein the dosage of the eluent is 1200mL, the eluent comprises methanol and acetic acid, and the volume ratio of the methanol to the acetic acid is 120:1, collecting eluate, and vacuum concentrating under reduced pressure to obtain Galla Turcica extract with gallic acid content of 108.2mg g -1 。
The preparation method of the vinyl pyrrolidone-maleic anhydride copolymer comprises the following steps:
adding 98g of maleic anhydride, 111g of 1-vinyl-2-pyrrolidone, 0.5g of azobisisobutyronitrile and 12g of divinylbenzene into a mixed solvent consisting of 500mL of dipropylene glycol dimethyl ether and 500mL of ethyl acetate, stirring and mixing uniformly, introducing nitrogen to replace air and protect the reaction, heating to 70 ℃, reacting for 10 hours, naturally cooling to room temperature, adding 1500mL of ethanol, stirring for 15 hours, filtering, performing Soxhlet purification on the obtained product with acetone for 48 hours, washing off unreacted monomers, finally drying in vacuum at 50 ℃ to constant weight, and crushing.
The preparation method of the toothpaste based on the nutgall extract comprises the following steps:
the preparation method comprises the following steps of uniformly mixing polyethylene glycol, sodium lauryl sulfate, cocamidopropyl betaine, a nutgall extract, a vinyl pyrrolidone-maleic anhydride copolymer, water and other auxiliary materials, adding the mixture into a paste preparation pot, adding powdered zinc citrate, sodium fluoride, anhydrous calcium pyrophosphate and xanthan gum, stirring and grinding the mixture, transferring the mixture into a storage pot, defoaming the mixture in vacuum, aging the mixture for 48 hours, and filling the mixture into a pipe.
Hydroxyapatite which is close to enamel of a human body is selected, the hydroxyapatite is smoked by cigarettes to obtain a tooth staining model with the color level of A4, the tooth staining model is put into 100mL of a 2% (mass fraction) toothpaste aqueous solution, the stirring speed is 400r/min, and the stain removing effect is compared after the room temperature treatment for 14 days, and the result is shown in figure 1, so that the toothpaste prepared by the embodiment has a good stain removing effect.
Example 2:
the toothpaste based on the nutgall extract comprises the following components in parts by weight:
10 parts of polyethylene glycol, 1.2 parts of sodium lauryl sulfate, 2 parts of xanthan gum, 0.8 part of zinc citrate, 0.5 part of cocamidopropyl betaine, 5 parts of nutgall extract, 0.15 part of sodium fluoride, 30 parts of anhydrous calcium pyrophosphate, 2 parts of vinylpyrrolidone-maleic anhydride copolymer and 20 parts of water.
The nutgall extract and the vinylpyrrolidone-maleic anhydride copolymer were prepared in the same manner as in example 1;
the preparation method of the toothpaste based on the nutgall extract comprises the following steps:
the preparation method comprises the steps of uniformly mixing polyethylene glycol, sodium lauryl sulfate, cocamidopropyl betaine, a nutgall extract, a vinyl pyrrolidone-maleic anhydride copolymer, water and other auxiliary materials, adding the mixture into a paste making pot, adding powdered zinc citrate, sodium fluoride, anhydrous calcium pyrophosphate and xanthan gum, stirring, grinding, transferring the mixture into a storage pot, defoaming in vacuum, aging for 48 hours, and filling the mixture into a pipe.
Example 3:
the toothpaste based on the nutgall extract comprises the following components in parts by weight:
5 parts of polyethylene glycol, 0.5 part of sodium lauryl sulfate, 1 part of xanthan gum, 0.2 part of zinc citrate, 0.1 part of cocamidopropyl betaine, 2 parts of nutgall extract, 0.05 part of sodium fluoride, 15 parts of anhydrous calcium pyrophosphate, 1 part of vinylpyrrolidone-maleic anhydride copolymer and 15 parts of water.
The nutgall extract and the vinylpyrrolidone-maleic anhydride copolymer were prepared in the same manner as in example 1;
the preparation method of the toothpaste based on the nutgall extract comprises the following steps:
the preparation method comprises the following steps of uniformly mixing polyethylene glycol, sodium lauryl sulfate, cocamidopropyl betaine, a nutgall extract, a vinyl pyrrolidone-maleic anhydride copolymer, water and other auxiliary materials, adding the mixture into a paste preparation pot, adding powdered zinc citrate, sodium fluoride, anhydrous calcium pyrophosphate and xanthan gum, stirring and grinding the mixture, transferring the mixture into a storage pot, defoaming the mixture in vacuum, aging the mixture for 24 hours, and filling the mixture into a pipe.
Example 4:
the toothpaste based on the nutgall extract comprises the following components in parts by weight:
10 parts of polyethylene glycol, 0.5 part of sodium lauryl sulfate, 2 parts of xanthan gum, 0.2 part of zinc citrate, 0.5 part of cocamidopropyl betaine, 2 parts of nutgall extract, 0.15 part of sodium fluoride, 15 parts of anhydrous calcium pyrophosphate, 2 parts of vinylpyrrolidone-maleic anhydride copolymer and 15 parts of water.
The nutgall extract and the vinylpyrrolidone-maleic anhydride copolymer were prepared in the same manner as in example 1;
the preparation method of the toothpaste based on the nutgall extract comprises the following steps:
the preparation method comprises the steps of uniformly mixing polyethylene glycol, sodium lauryl sulfate, cocamidopropyl betaine, a nutgall extract, a vinyl pyrrolidone-maleic anhydride copolymer, water and other auxiliary materials, adding the mixture into a paste making pot, adding powdered zinc citrate, sodium fluoride, anhydrous calcium pyrophosphate and xanthan gum, stirring, grinding, transferring the mixture into a storage pot, defoaming in vacuum, aging for 48 hours, and filling the mixture into a pipe.
Example 5:
the toothpaste based on the nutgall extract comprises the following components in parts by weight:
5 parts of polyethylene glycol, 1.2 parts of sodium lauryl sulfate, 1 part of xanthan gum, 0.8 part of zinc citrate, 0.1 part of cocamidopropyl betaine, 5 parts of nutgall extract, 0.05 part of sodium fluoride, 30 parts of anhydrous calcium pyrophosphate, 1 part of vinylpyrrolidone-maleic anhydride copolymer and 20 parts of water.
The nutgall extract and the vinylpyrrolidone-maleic anhydride copolymer were prepared in the same manner as in example 1;
the preparation method of the toothpaste based on the nutgall extract comprises the following steps:
the preparation method comprises the steps of uniformly mixing polyethylene glycol, sodium lauryl sulfate, cocamidopropyl betaine, a nutgall extract, a vinyl pyrrolidone-maleic anhydride copolymer, water and other auxiliary materials, adding the mixture into a paste making pot, adding powdered zinc citrate, sodium fluoride, anhydrous calcium pyrophosphate and xanthan gum, stirring, grinding, transferring the mixture into a storage pot, defoaming in vacuum, aging for 24 hours, and filling the mixture into a pipe.
Comparative example 1:
substantially the same as in example 1, except that a commercially available nutgall extract was used in place of the nutgall extract prepared in the present invention.
Comparative example 2:
essentially the same as in example 1, except that no vinylpyrrolidone-maleic anhydride copolymer was added.
And (3) performance testing:
the toothpaste prepared in example 1 of the present invention and comparative examples 1 and 2 was used as a sample for performance test;
culturing streptococcus mutans, gingival cremopsis monalis, staphylococcus aureus and escherichia coli to form a mixed bacteria biomembrane, preparing a sample into a suspension with the mass concentration of 0.5g/L by using sterile water, adding 1mL of the suspension into a pore of a biomembrane pore plate, keeping for 3min, lightly washing for 3 times (1 mL/time) by using normal saline, continuously culturing the biomembrane, changing the solution once every 1h, namely sucking all the solution of the system, adding 1mL of brain and heart infusion Broth (BHI) enrichment culture medium, and respectively carrying out viable count on the biomembrane at the bottom of the pore by using a flat viable count method at 0,4h and 8 h.
The test results are shown in table 1 below:
table 1:
as can be seen from the above table 1, the toothpaste prepared by the invention has long-acting and durable antibacterial performance, and the addition of the vinylpyrrolidone-maleic anhydride copolymer plays a positive role in improving the long-acting antibacterial performance of the toothpaste.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The toothpaste based on the nutgall extract is characterized by comprising the following components:
polyethylene glycol, sodium lauryl sulfate, xanthan gum, zinc citrate, cocamidopropyl betaine, nutgall extract, fluorine-containing inorganic salt, abrasive, vinyl pyrrolidone-maleic anhydride copolymer, water and other auxiliary materials.
2. The toothpaste based on the nutgall extract as claimed in claim 1, which comprises the following components in parts by weight:
5-10 parts of polyethylene glycol, 0.5-1.2 parts of sodium lauryl sulfate, 1-2 parts of xanthan gum, 0.2-0.8 part of zinc citrate, 0.1-0.5 part of cocamidopropyl betaine, 2-5 parts of nutgall extract, 0.05-0.15 part of fluorine-containing inorganic salt, 15-30 parts of abrasive, 1-2 parts of vinyl pyrrolidone-maleic anhydride copolymer, 15-20 parts of water and 0-6 parts of other auxiliary materials.
3. The toothpaste based on nutgall extract as claimed in claim 1, wherein the content of gallic acid in the nutgall extract is not less than 100mg g -1 。
4. The toothpaste based on a nutgall extract as claimed in claim 1, wherein said nutgall extract is prepared by the following method:
adding Galla Turcica medicinal powder into methanol water solution, extracting under the action of ultrasonic wave at 40-50 deg.C for 5-10 hr, filtering the extractive solution, extracting the residue again, mixing the extractive solutions, adding phenyl bonded silica gel into the extractive solution, mixing with dry method, loading into solid phase extraction column tube, compacting, eluting with peristaltic pump driven eluent, collecting eluate, and vacuum concentrating under reduced pressure.
5. The gallnut extract-based toothpaste according to claim 4, wherein said eluent comprises methanol and acetic acid, said methanol and acetic acid being present in a volume ratio of 100-120:1.
6. the toothpaste based on nutgall extract as claimed in claim 1, wherein said fluorine-containing inorganic salt is any one or more of sodium fluoride, potassium monofluorophosphate and stannous fluoride.
7. The gallnut extract-based toothpaste of claim 1, wherein said abrasive is any one or more of dibasic calcium phosphate dihydrate, calcite powder, precipitated silica, anhydrous calcium pyrophosphate, aluminum hydroxide, titanium dioxide.
8. The gallnut extract-based toothpaste of claim 1, wherein said vinylpyrrolidone-maleic anhydride copolymer is prepared as follows:
adding maleic anhydride, vinyl pyrrolidone, azodiisobutyronitrile and divinylbenzene into a mixed solvent consisting of dipropylene glycol dimethyl ether and ethyl acetate, stirring and mixing uniformly, introducing nitrogen for protection, heating to 65-75 ℃, reacting for 6-10h, naturally cooling to room temperature, adding ethanol, stirring for 10-20h, filtering, performing Soxhlet purification on the obtained product for 24-48h by using acetone, washing off unreacted monomers, finally performing vacuum drying to constant weight, and crushing.
9. The toothpaste based on nutgall extract as claimed in claim 1, wherein the other auxiliary materials comprise any one or more of buffering agent, humectant, food coloring agent, preservative, essence, sweetener, spice and western medicine components.
10. A process for preparing a toothpaste according to any one of claims 1 to 9 based on gallnut extract, wherein polyethylene glycol, sodium lauryl sulfate, cocamidopropyl betaine, gallnut extract, vinylpyrrolidone-maleic anhydride copolymer, water and other adjuvants are mixed uniformly, added into a paste preparation pot, then added with zinc citrate powder, fluorine-containing inorganic salt, abrasive and xanthan gum, stirred, ground, transferred into a storage pot for vacuum defoamation, aged for 24-48h and finally bottled.
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